CN104464893A - Small-blocking-agent-loaded graphene conductive slurry and preparation method and application thereof - Google Patents
Small-blocking-agent-loaded graphene conductive slurry and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses small-blocking-agent-loaded graphene conductive slurry and a preparation method and application of the small-blocking-agent-loaded graphene conductive slurry. The conductive slurry comprises 1wt% to 10 wt% of conductive components, 0.5 wt% to 8 wt% of dispersing agents and 85 wt% to 95 wt% of solvents. The conductive components comprise small-blocking-agent-loaded graphene serving as the basic conductive components and auxiliary conductive components. According to the slurry, small blocking agents are loaded on the graphene so that stacking among the graphene can be eliminated thoroughly, the processing difficulty of the graphene is lowered, the dispersity of the graphene in the conductive slurry is improved greatly, and thus the conductive slurry excellent in performance is obtained; according to electronic devices formed through the conductive slurry, especially energy storage devices, such as li-ion battery products which have excellent conductive performance and heat conducting performance, the power density, rate capacity, tap density, circulation stability, and other performance of the electronic devices are improved greatly, the service life of the electric devices is greatly prolonged, and the conductive slurry is simple in preparation process and low in cost.
Description
Technical field
The present invention relates to a kind of electrocondution slurry and preparation method thereof, particularly a kind of high connductivity Graphene slurry, its preparation method and application, belong to electrocondution slurry and conductive agent technical field.
Background technology
Along with lithium ion battery is in the increase of electrokinetic cell domain requirement, the internal resistance of cell is large, power density is low, cycle life is short, stability is low, easy heating produces the problems such as security incident and day by day highlights also urgently to be resolved hurrily.Wherein, positive electrode Mn oxide, the material electric conductivities such as phosphate are all very low, but also will keep good high rate charge-discharge characteristic, longer useful life, and this is the industrial huge challenge faced of current driving force lithium ion battery just.The conductivity of negative pole graphite material is slightly good, but in repeatedly discharge and recharge, the dilation of graphite material, contact between graphite granule is reduced, gap increases, and even some departs from collector electrode, becomes dead active material, no longer participate in electrode reaction, so also need to add conductive agent to keep the stable of the negative material conductivity in cyclic process.As the conductive agent (accounting for 5-10wt% in pole piece) of lithium ion battery important component part, there is important effect to improving battery performance.The research and development of novel conductive agent of charge-discharge magnification, cyclical stability can be improved, become an important topic of Study on Li-ion batteries.
Graphene (Graphene) is the Two-dimensional Carbon nano structural material that mono-layer graphite sheet is formed, and Graphene has excellent mechanics, electricity and thermal property.The mobility of Graphene can reach 2 × 10
4cm
2/ V × s is 100 times of silicon, and at room temperature the resistivity of Graphene can reach 10
8s/m, can tolerate is 10
8the electric current of A/cm2, be 100 times of copper tolerance, thermal conductivity is 3000-5000W/mK, can match in excellence or beauty with diamond, and specific area can reach 2630m
2/ g.The performance of these excellences of Graphene has wide practical use in the field such as lithium ion battery, ultracapacitor, has also caused the extensive concern of scientific circles and industrial quarters.Find that therefore two scientists of Graphene obtain Nobel Prize in physics in 2010.Preparation method determines the performance of material.At present, the preparation method of development graphite alkene powder comprises: chemistry redox method, organic synthesis method, intercalation plavini, and liquid phase cleavage method etc.A large amount of preparations of Graphene are also limited to the approach restored by chemical oxidation and realize, and not yet form ripe industrialization production and application.But restore method by chemical oxidation, Graphene modified multiple functional group and produced a large amount of defect, in electricity, the multiple aspect of performance such as calorifics is worse than the Graphene of intrinsic far away, greatly limit the practical application of Graphene.Therefore, by the improvement of graphene preparation method, obtaining a large amount of, low cost, the high-quality graphene of high connductivity, high heat conduction, will be the inexorable trend of Graphene preparation of industrialization development, is also the basis in early stage of Graphene application in conduction, heat conduction.In addition, due to large specific area, very easily there is irreversible stacking in Graphene in the course of processing, makes the dispersiveness of Graphene poor, limit the performance of Graphene high connductivity, high thermal conductivity.
Summary of the invention
Main purpose of the present invention is graphene conductive slurry providing a kind of load small size barrier and preparation method thereof, in this electrocondution slurry, Graphene is without stacking, favorable dispersibility, conductivity is high, greatly can improve electronic device, the particularly conduction, heat conduction, energy-storage property etc. of energy storage device, thus overcome defect of the prior art.
Another object of the present invention is to the application of the graphene conductive slurry that described load small size barrier is provided.
For realizing aforementioned invention object, the technical solution used in the present invention comprises:
A graphene conductive slurry for load small size barrier, comprising: conductive component 1wt%-10wt%, dispersant 0.5wt%-8wt% and solvent 85wt%-95wt%;
Wherein, described conductive component comprises Graphene as the load small size barrier of basic conductive component and additional conductive component, and the mass ratio of described basic conductive component and additional conductive component is 1:5-5:1.
As one of comparatively preferred embodiment, described Graphene is the high-quality graphene of basic zero defect, free from admixture and functional group.
Further, the number of plies of described Graphene is 1-25 layer, and lamella is of a size of 500nm-20 μm.
Further, described small size barrier can preferably from but be not limited to that carbon black, acetylene black, Ketjen black, carbon fiber, carbon are brilliant, the combination of any one or more in electrically conductive graphite and carbon nano-tube.
Further, described small size barrier is supported between graphene layer with the form of physical absorption.
Further, described small size barrier is of a size of 10nm-5 μm.
Further, the mass ratio of described small size barrier and Graphene is 1:20-10:1.
Further, described additional conductive component can preferably from but be not limited to that acetylene black, Ketjen black, carbon fiber, carbon are brilliant, the combination of any one or more in electrically conductive graphite and carbon nano-tube.
Further, described dispersant can preferably from but the combination of any one or more be not limited in polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, butadiene-styrene rubber, sodium carboxymethylcellulose, cetyl ammonium bromide, dodecyl sodium sulfate, neopelex, Kynoar, polytetrafluoroethylene Triton-100, tween.
Further, described solvent can preferably from but be not limited to the combination of any one or more in DMF, isopropyl alcohol, butyl acetate, 1-METHYLPYRROLIDONE, water.
The preparation method of the graphene conductive slurry of described load small size barrier, comprising:
A, Graphene, small size barrier and solvent or solvent and dispersant are evenly formed the first slurry, the hybrid mode wherein adopted comprises the mixing of solvent, mechanical mixture or air-flow;
B, by the first slurry and additional conductive component or additional conductive component and dispersant and vacuum stirring obtains the second slurry;
C, by the second slurry sand mill 2-7h, 100-500 mesh sieve, obtain described graphene conductive slurry.
The graphene conductive slurry of described load small size barrier is in preparing the application in electronic device, and described electronic device comprises energy storage device, and described energy storage device comprises lithium ion battery or ultracapacitor.
A kind of device, comprises the conductive structure formed by the graphene conductive slurry of described load small size barrier.
Compared with prior art, beneficial effect of the present invention comprises: by load small size barrier on Graphene, the stacking between Graphene can be stopped, reduce the difficulty of processing of Graphene, the dispersiveness of Graphene in electrocondution slurry is significantly improved, thus obtain the electrocondution slurry of excellent performance, utilize the electronic device that this electrocondution slurry is formed, particularly energy storage device, such as lithium electricity product has excellent conductive, heat conductivility, and its power density, rate capability, tap density, cyclical stability, the performances such as useful life also have significantly to be improved, and this electrocondution slurry processing technology is simple, with low cost.
Accompanying drawing explanation
Fig. 1 is the structural representation of the Graphene of a kind of typical load lock agent in the present invention;
Fig. 2 is preparation technology's flow chart of a kind of high connductivity Graphene slurry among a kind of typical embodiments in the present invention;
Fig. 3 is the SEM figure of the graphene powder of the load carbon black formed by solvent in embodiment 1;
Fig. 4 is that in embodiment 1, high connductivity Graphene slurry is coated in the SEM figure on aluminium foil;
Fig. 5 is embodiment 1, reference examples 1 slurry and LiFePO4 composite membrane conducting trace comparison diagram on PET;
The lithium electricity high rate performance comparison diagram of the pole piece that Fig. 6 is embodiment 2, reference examples 2 slurry and LiFePO4 are compounded to form.
Embodiment
One aspect of the present invention provides a kind of graphene conductive slurry of load small size barrier, and it is preferably made up of conductive component (1wt%-10wt%), dispersant (0.5wt%-8wt%) and solvent (85wt%-95wt%).
Wherein, conductive component is preferably made up of the basic conductive component of Graphene of load small size barrier and additional conductive component.
Among a typical embodiments, the structure of the Graphene of load small size barrier can consult Fig. 1.
Another aspect of the present invention provides a kind of preparation method of graphene conductive slurry of load small size barrier, and refer to Fig. 2, among a typical embodiments, it comprises the steps:
A, Graphene, small size barrier to be mixed with solvent (dispersant), obtain the first slurry;
B, the first slurry and additional conductive component, dispersant vacuum stirring are obtained the second slurry;
C, by second slurry sand mill, sieving obtains final high connductivity Graphene slurry.
Below in conjunction with some embodiments and accompanying drawing, technical scheme of the present invention is further described.
Embodiment 1:
(average thickness is 3nm, and average chip size is 20 μm, and dry powder becomes membrane conductivity average out to 10 to get 30g high-quality graphene powder
5s/m) stir ultrasonic 1h in ethanol with 10g carbon black, mix the graphene powder (as Fig. 3) that rear 80 DEG C of oven dry obtain adsorption carbon black.After this powder and 10g KS-6,50g PVDF, 900g NMP are stirred 3h in vacuum planetary mixer, in sand mill, grind 2h, cross the oiliness high-conductivity slurry that 200 mesh sieves obtain carbon containing 5wt%.This high-conductivity slurry is coated the film pattern of aluminium foil surface formation as Fig. 4.
Embodiment 2:
(average thickness is 3nm, and average chip size is 20 μm, and dry powder becomes membrane conductivity average out to 10 to get 30g high-quality graphene powder
5s/m) stir ultrasonic 1h in ethanol with 10g 10000 order graphite, mix the graphene powder that rear 80 DEG C of oven dry obtain adsorption carbon black.After this powder and 10g CNTs, 300g LA132 binding agent, 650g water are stirred 3h in vacuum planetary mixer, in sand mill, grind 2h, cross the water-based high-conductivity slurry that 200 mesh sieves obtain carbon containing 5wt%.
Reference examples 1: this reference examples is substantially identical with embodiment 1 (example 1 namely in figure), but defines electrocondution slurry with the graphene powder that graphene powder replaces surperficial adsorbent charcoal black.The active slurry that this slurry and LiFePO4 are mixed to form is applied to PET upper surface, it is seen, the film (thickness is 20 μm) (as Fig. 5) that the composite mortar of the slurry that its resistivity is prepared in embodiment 1 and LiFePO4 is formed.
Reference examples 2: this reference examples is substantially identical with embodiment 2 (example 2 namely in figure), but defines electrocondution slurry with the graphene powder that carbon black replaces surperficial adsorbent charcoal black.The active slurry that this slurry and LiFePO4 are mixed to form is applied to the pole piece that aluminium foil is formed and is assembled into lithium ion battery, and contrast with the slurry prepared in embodiment 2, can see that its high rate performance obviously reduces (as Fig. 6).
Above-described embodiment has been described in detail technical scheme of the present invention and beneficial effect; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; all any amendments and improvement etc. made in spirit of the present invention, all should be included within protection scope of the present invention.
Claims (10)
1. a graphene conductive slurry for load small size barrier, is characterized in that comprising: conductive component 1wt%-10wt%, dispersant 0.5wt%-8wt% and solvent 85wt%-95wt%; Wherein said conductive component comprises Graphene as the load small size barrier of basic conductive component and additional conductive component, and the mass ratio of described basic conductive component and additional conductive component is 1:5-5:1.
2. the graphene conductive slurry of load small size barrier according to claim 1, it is characterized in that described Graphene is the high-quality graphene of basic zero defect, free from admixture and functional group, and the number of plies of described Graphene is 1-25 layer, lamella is of a size of 500nm-20 μm.
3. the graphene conductive slurry of load small size barrier according to claim 1, it is characterized in that described small size barrier is supported between graphene layer with the form of physical absorption, described small size barrier comprises the combination of any one or more in carbon black, acetylene black, Ketjen black, carbon fiber, carbon crystalline substance, electrically conductive graphite and carbon nano-tube, and the size of described small size barrier is 10nm-5 μm.
4. the graphene conductive slurry of load small size barrier according to claim 1, is characterized in that the mass ratio of described small size barrier and Graphene is 1:20-10:1.
5. the graphene conductive slurry of load small size barrier according to claim 1, is characterized in that described additional conductive component comprises the combination of any one or more in acetylene black, Ketjen black, carbon fiber, carbon crystalline substance, electrically conductive graphite and carbon nano-tube.
6. the graphene conductive slurry of load small size barrier according to claim 1, is characterized in that described dispersant comprises the combination of any one or more in polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, butadiene-styrene rubber, sodium carboxymethylcellulose, cetyl ammonium bromide, dodecyl sodium sulfate, neopelex, Kynoar, polytetrafluoroethylene Triton-100, tween.
7. the graphene conductive slurry of load small size barrier according to claim 1, is characterized in that described solvent comprises the combination of any one or more in DMF, isopropyl alcohol, butyl acetate, 1-METHYLPYRROLIDONE, water.
8. the preparation method of the graphene conductive slurry of load small size barrier according to any one of claim 1-7, is characterized in that comprising:
A, Graphene, small size barrier and solvent or solvent and dispersant are evenly formed the first slurry, the hybrid mode wherein adopted comprises the mixing of solvent, mechanical mixture or air-flow;
B, by the first slurry and additional conductive component or additional conductive component and dispersant and vacuum stirring obtains the second slurry;
C, by the second slurry sand mill 2-7h, 100-500 mesh sieve, obtain described graphene conductive slurry.
9. the graphene conductive slurry of the load small size barrier according to any one of claim 1-7 is in preparing the application in electronic device, and described electronic device comprises energy storage device, and described energy storage device comprises lithium ion battery or ultracapacitor.
10. a device, is characterized in that the conductive structure that the graphene conductive slurry of the load small size barrier comprised according to any one of claim 1-7 is formed.
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| CN105006268A (en) * | 2015-06-19 | 2015-10-28 | 周焕民 | Method for preparing solid-phase graphene conductive dispersion |
| CN105633359A (en) * | 2016-03-25 | 2016-06-01 | 山东精工电子科技有限公司 | Preparation method for negative electrode paste with high-rate discharging performance, and negative electrode pole piece |
| CN106450333A (en) * | 2016-10-28 | 2017-02-22 | 合肥国轩电池材料有限公司 | Lithium battery anode slurry and slurry mixing method thereof |
| CN106433319A (en) * | 2016-10-14 | 2017-02-22 | 中国科学院山西煤炭化学研究所 | Waterborne environment-friendly conducive carbon paste based on graphene-carbon black composite filler and preparation method |
| CN106654204A (en) * | 2016-12-15 | 2017-05-10 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for graphene conductive slurry |
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| CN108039225A (en) * | 2017-12-13 | 2018-05-15 | 常州烯材碳材料科技有限公司 | Environment-friendly type low resistance graphene carbon fiber conductive carbon paste and preparation method thereof |
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| CN109455707A (en) * | 2018-12-27 | 2019-03-12 | 宁波杉元石墨烯科技有限公司 | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion |
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| CN105633359A (en) * | 2016-03-25 | 2016-06-01 | 山东精工电子科技有限公司 | Preparation method for negative electrode paste with high-rate discharging performance, and negative electrode pole piece |
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| CN106784827A (en) * | 2016-12-19 | 2017-05-31 | 中国科学院电工研究所 | Mesoporous graphene conductive slurry and Preparation method and use |
| CN107180667A (en) * | 2017-04-28 | 2017-09-19 | 北京北方国能科技有限公司 | A kind of electrocondution slurry and preparation method thereof, application |
| CN109256283A (en) * | 2017-07-13 | 2019-01-22 | 山东欧铂新材料有限公司 | A kind of conductive agent and preparation method thereof for supercapacitor |
| CN109256283B (en) * | 2017-07-13 | 2021-05-18 | 山东欧铂新材料有限公司 | Conductive agent for super capacitor and preparation method thereof |
| CN107799204A (en) * | 2017-10-18 | 2018-03-13 | 温州市赢创新材料技术有限公司 | A kind of touch-screen graphene conductive film and preparation method thereof |
| CN107799204B (en) * | 2017-10-18 | 2019-04-09 | 温州市赢创新材料技术有限公司 | A kind of touch screen graphene conductive film and preparation method thereof |
| CN108023059A (en) * | 2017-11-30 | 2018-05-11 | 东莞市金源电池科技有限公司 | A kind of process for dispersing of lithium battery slurrying graphene |
| CN108039225A (en) * | 2017-12-13 | 2018-05-15 | 常州烯材碳材料科技有限公司 | Environment-friendly type low resistance graphene carbon fiber conductive carbon paste and preparation method thereof |
| CN108211828A (en) * | 2017-12-28 | 2018-06-29 | 清华大学 | A kind of method for preparing graphene/carbon nanotube hybrid object carbon slurry |
| CN108211828B (en) * | 2017-12-28 | 2020-08-18 | 清华大学 | Method for preparing graphene carbon nanotube hybrid carbon slurry |
| CN108736004A (en) * | 2018-05-31 | 2018-11-02 | 深圳市瑞达电源有限公司 | A kind of anode diachylon for lead-acid accumulator |
| CN109455707A (en) * | 2018-12-27 | 2019-03-12 | 宁波杉元石墨烯科技有限公司 | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion |
| CN109935806A (en) * | 2019-02-25 | 2019-06-25 | 天津艾克凯胜石墨烯科技有限公司 | A kind of graphene composite conductive slurry and preparation method thereof for lithium ion battery |
| CN110518196A (en) * | 2019-07-11 | 2019-11-29 | 高芳 | A kind of negative electrode material of lithium battery |
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